麦冬类药材的甄别以及质量与安全性评价

【作者】 孟淼；

【导师】 孙毅坤；

【作者基本信息】 北京中医药大学 ， 中医学， 2010， 硕士

【摘要】 麦冬,原名麦门冬,为我国传统医药常用的清热、养阴、润燥药,适用于阴虚内热、津枯口渴及气逆、燥咳痰稠,或热病伤津、便秘等症。《中华人民共和国药典》从2000年版开始,将麦冬类药材分别收载为麦冬和山麦冬二种,功能主治皆略有不同。麦冬为百合科沿阶草属植物麦冬Ophiopogon japonicus (Thunb.)Ker-Gawl.的干燥块根,又根据产地的不同分为川麦冬和杭麦冬。山麦冬为百合科植物山麦冬属植物湖北麦冬Liriope spicata (Thunb.) Lour. Var. prolifera Y. T. Ma或短葶山麦冬Liriope muscari (Decne.)Baily的干燥块根。这几种药材虽然外形相似,极易混淆,但药效不同,质量不同,价格也不尽相同。目前,在药材市场中,许多不法商贩以次充好,以假乱真,或者真伪掺杂,这对于个人乃至在实际生产中都会造成较大的困扰,而至今为止的麦冬鉴别文献中,所选用的药材大部分都是直接来源于药材产区,不存在以次充好、真伪掺杂的市场问题,以此为基础所得出的结论,无法解决实际生产中麦冬品种混淆的问题。本研究通过对麦冬类药材的甄别以及质量与安全性的评价,可以准确、便捷的辨别市售麦冬的种类,并确立质量评价与安全性评价依据,解决大生产中无法确定市售麦冬品种的问题。1.对麦冬类药材分别进行性状、显微、荧光、薄层色谱、HPLC鉴别,其中性状、显微、荧光鉴别法对于麦冬类药材的甄别意义不大,而薄层、液相鉴别可以较好的区分麦冬类药材。2.采用高效液相色谱法,分别对麦冬类药材中的甲基麦冬黄烷酮A、B以及麦冬皂苷C进行含量测定,同时进行了方法学考察,结果表明该方法准确,重现性好,回收率分别为101.67%,RsD=0.63%；103.67%,RSD=2.4%；100.87%,RsD=2.3%。通过对麦冬类药材中的甲基麦冬黄烷酮A、B以及麦冬皂苷C的定量分析,对麦冬类药材进行质量评价,从定性与定量两方面,对麦冬类药材进一步做出甄别。3.采用气相色谱-质谱联用法(GC-MS法)同时对麦冬类药材中乐果、二嗪农、甲基对硫磷、马拉硫磷、对硫磷、杀扑磷6种常用有机磷类农药进行定性及定量分析。结果：标准工作曲线的相关系数在0.992～0.997,加样回收率在75.44%～128.75%之间,相对标准偏差小于17%,符合农药残留分析的要求。15份不同种类麦冬类药材中有机磷农药残留均未超过国家标准。结论：本方法选择性好、重现性好、灵敏度高,可用于不同种类麦冬类药材中有机磷类农药残留量的检测。本研究以性状、显微、荧光、薄层色谱、HPLC鉴别为手段,对麦冬类药材进行甄别；建立以甲基麦冬黄烷酮A、B以及麦冬皂苷C为指标的定量分析方法,对麦冬类药材进行质量评价,对麦冬类药材进一步做出甄别；建立麦冬类药材中6种常用有机磷农药的定性及定量分析方法,对麦冬类药材进行安全性评价。更多还原

【Abstract】 Ophiopogon japonicus, used to be called Ophiopogon, is a kind of Chinese traditional medicine commonly used for the heat, nourishing yin, moistening agents which is applicable to deficiency heat, thirst and dry air reverse Tianjin, dry thick sputum, or fever disability allowance, constipation embolism. It is set separately two kinds of ophiopogon japonicus and liriope with slightly different attending functions in《The People’s Republic of China Pharmacopoeia》, the 2000 edition. Ophiopogon japonicus is the dried root of the Ophiopogon japonicus which belongs to the Liliaceae Ophiopogon species named Chuan ophiopogon japonicus and Hang ophiopogon japonicus according to its place of origin while liriope is the dried root of the hyacinth liriope, ophiopogon japonicus plants in Hubei or short ting liriope.These types of medicinal herbs are easily confused for their similar shape, but they are quite different in their efficacy, quality and price. In the present herbal medicine market some illegal traders mix the spurious with the genuine by many means which brings much trouble to consumers and actual production. Until now the conclusion from our distinction articles can’t help us to solve the problem of definiting the ophiopogon species because their chosen herbs are directly from their medicine production area, without such mixture as in the present market mentioned above.The research suggests we can easily distinguish the variety of the ophiopogon sold in the market by screening and evaluation of quality and safety so as to solve the problem we meet in the production.1. Distinguish the ophiopogon japonicus by character, shape, micro, fluorescence,HPLC, and thin layer, and the last method is better but the fluorescent identification method is of little significance.2. Determine its content of methyl ophiopogon flavanone A,B and ophiopogon japonicus saponin C with the method of highly effective liquid phase chromatography and at the meantime investigate the methodology to prove its validity with good reproduction quality and its returns-ratio respectively is 101.67%, RSD=0.63%; 103.67%, RSD=2.4%; 100.87%, RSD=2.3%.By the quantitative analysis, give the quality evaluation to make further screening from the two aspects of quality and quantity.3. Analyse the quality and quantity of its six kinds of common organophosphate pesticides as dimethoate, diazinon, methyl parathion, malathion, parathion and methidathion with method of gas chromatography-mass spectrum joint usage. No organophosphorus pesticide residues have been detected out of 15 samples. The correlation coefficient of standard working curve is between 0.992-0.997, the type adding returns-ratio is between 75.44%～128.75%, the relative standard deviation is lower than 17%,and all these agree to the requirements for pesticide residue analysis. The organophosphorus pesticide residues of the 15 different types of ophiopogon japonicus do not exceed our national standards.Conclusion:The method can be used to detect organophosphorus pesticide residues in different types of ophiopogon japonicus with its selectivity, good reproducibility and high sensitivity.The resarech studies screening ophiopogon japonicus herbs by means of character, shape, micro, fluorescence, HPLC,and thin layer, giving the quality Evaluation with the method of quantitative Analysis taking ophiopogon flavanone methyl A, B, and ophiopogon japonicus saponin C as an index, making further screening on the types of ophiopogon japonicus, and giving safety evaluation on them by establishing qualitative and quantitative analysis methods on 6 kinds of commonly used organophosphorus pesticides.更多还原